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WO2000075075A1 - Enrichissement du zircon - Google Patents

Enrichissement du zircon Download PDF

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Publication number
WO2000075075A1
WO2000075075A1 PCT/ZA2000/000104 ZA0000104W WO0075075A1 WO 2000075075 A1 WO2000075075 A1 WO 2000075075A1 ZA 0000104 W ZA0000104 W ZA 0000104W WO 0075075 A1 WO0075075 A1 WO 0075075A1
Authority
WO
WIPO (PCT)
Prior art keywords
afdz
zirconium
zbs
residue
zircon
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/ZA2000/000104
Other languages
English (en)
Inventor
Willem Johannes De Wet
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Coetzee Gert Hendrik Jacobus
University of Pretoria
Original Assignee
Coetzee Gert Hendrik Jacobus
University of Pretoria
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Coetzee Gert Hendrik Jacobus, University of Pretoria filed Critical Coetzee Gert Hendrik Jacobus
Priority to US10/009,110 priority Critical patent/US7063824B1/en
Priority to AU56437/00A priority patent/AU5643700A/en
Publication of WO2000075075A1 publication Critical patent/WO2000075075A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G25/00—Compounds of zirconium
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G25/00—Compounds of zirconium
    • C01G25/02—Oxides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G25/00—Compounds of zirconium
    • C01G25/06—Sulfates
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B1/00—Preliminary treatment of ores or scrap
    • C22B1/02—Roasting processes
    • C22B1/06—Sulfating roasting
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B34/00—Obtaining refractory metals
    • C22B34/10—Obtaining titanium, zirconium or hafnium
    • C22B34/14—Obtaining zirconium or hafnium

Definitions

  • This invention relates to a process of treating zirconium containing products
  • the method including beneficiating zircon to increase the zirconium content thereof.
  • invention also relates to products of such a process including zircon derived
  • opacifier material suitable for pigments and including opacifier material.
  • zirconium Before zirconium can be retrieved from zircon sand, the zircon sand needs to
  • Thermal decomposition entails
  • Chemical decomposition can be achieved by reacting zircon with a source of
  • alkali-fusion decomposed zircon product (hereinafter referred to as alkali-fusion decomposed zircon product or AFDZ).
  • the AFDZ may be treated in a number of ways namely:
  • a common way of beneficiating zircon comprises reacting zircon with sodium
  • ZBS (hereinafter referred to as ZBS) with the formula ZrsO ⁇ SO ⁇ .
  • Precipitation is usually from
  • Zircon also has a natural radioactive content with associated occupational
  • ZBS sulphate
  • AFDZ formed from reacting zircon with a source of alkali
  • alkali metal includes, in addition to its normal
  • alkali metal ions and compounds including such ions.
  • the process may also include reacting zircon with a source of alkali metal at
  • the forming of the AFDZ may
  • the ZBS may be used as formed.
  • the ZBS may be used as formed.
  • the ZBS may be purified.
  • a major advantage of this process is that the ZBS may be purified.
  • the ZBS is a solid which
  • radio active species can be removed from the ZBS containing residue
  • hydrated zirconium oxide are both hydrated zirconium products.
  • AFDZ may be formed by leaching the AFDZ to provide a leachate containing non-
  • the AZST may be formed by reacting the AFDZ with
  • the AZST that forms in both the above processes is in a solid form which may be dried, preferably at
  • the AZST containing solid may then be leached (preferably with
  • the hydrated ZBC may be formed
  • hydrated zirconium oxide may be formed by adding NH 3 to the AZST.
  • hydrated zirconium product(s) which form are preferably washed (preferably
  • the hydrated zirconium product may be formed by leaching the
  • the solid hydrated zirconium product may be treated with a source sulphate
  • zircon to increase the zirconium content thereof comprises the steps of:
  • the AFDZ which forms contain acid extractable zirconium which remains in
  • radio active species can be removed from the ZBS containing residue, leaving
  • the process may include the step of forming AFDZ by reacting zircon with
  • a source of alkali metal at elevated temperatures Preferably the source of
  • alkali metal comprises an alkali metal containing compound and preferably it
  • the alkali metal containing compound comprises a sodium containing compound.
  • the compound comprises NaOH or Na 2 C0 3 .
  • the zircon and NaOH may be allowed to react in a C0 2 -free
  • the AFDZ is preferably leached with water.
  • the leachate contains
  • AFDZ can be given as follows (for X 2):
  • zircon at 650°C. At fusion temperatures of 850°C more zirconium is acid
  • the zirconium species in the wet residue comprise ZrO 2 .xH 2 0 (from
  • the wet residue is preferably treated with a
  • the zircon and the alkali metal containing compound may be mixed in a mass
  • metal containing compound is Na 2 C0 3 , the mass ratio is typically between 1:
  • 0,4 and 1: 0,7 preferably between 1: 0,58 and 1:0,66 e.g. about 1: 0,65.
  • the alkali metal containing compound is NaOH, the mass ratio is typically
  • the elevated temperature is preferably
  • the alkali metal containing compound is Na 2 C0 3 , the
  • elevated temperature is preferably between 900°C and 1300°C, and more
  • the zircon is in particulate form when reacting with the alkali metal
  • the method may thus include subjecting raw zircon
  • a suitable d 50 particle size for the alkali metal containing compound as the alkali metal containing compound, a suitable d 50 particle size for the
  • zircon is between lO ⁇ m and 45 ⁇ m.
  • a suitable d 50 particle size for the zircon is between 5 ⁇ m and lO ⁇ m.
  • the AFDZ Prior to subjecting the AFDZ to the leaching step, the AFDZ may be cooled
  • the AFDZ is comminuted to a d 50 particle size
  • the leaching step may be a water leaching or water washing step.
  • alkali metal containing compound is NaOH, at least some silica present in the
  • AFDZ will be leached from the AFDZ.
  • present in the AFDZ is leached out into the water. More preferably, at least
  • silica 60% of the silica is leached out into the water, and typically at least 66%> of the silica is leached out into the water.
  • precipitated silicas may be produced from the leachate by methods known to
  • the residue formed after the leaching step is wet and usually includes some
  • alkali metal therein. At least some of the alkali metal may be recovered from
  • compound used is NaOH, recovering at least some of the alkali from the wet
  • residue may include mixing NaHC0 3 with the wet residue formed after
  • the NaHC0 3 may be mixed in a stoichiometric quantity
  • Na 2 C0 3 recovered may be in the form of a concentrated Na 2 C0 3 solution
  • Na 2 C0 3 may advantageously be precipitated as NaHC0 3 for re- use or be sold as a byproduct.
  • alkali metal comprises sodium
  • present is converted to NaHC0 3 which upon
  • the residue Prior to preparing the ZBS the residue is preferably acidified or neutralised,
  • Acid such as hydrochloric acid or
  • sulphuric acid may be used for this purpose and preferably only hydrochloric
  • the residue may also be washed or leached, e.g. with water, to remove non-
  • alkali metal species such as sodium salts
  • AFDZ may be acidified or neutralised and the resulting product is then
  • Hydrochloric acid or sulphuric acid may be used for
  • hydrochloric acid preferably only hydrochloric acid.
  • it is acidified or
  • the main purposes of leaching the AFDZ is to reduce the alkali metal content
  • the leached products can be exploited for by-product manufacture.
  • the ZBS may be formed by adding a stoichiometric quantity of a source of
  • sulphate preferably H 2 S0 4 or acid zirconium sulphate tetrahydrate (AZST) to
  • the wet ZBS-containing residue may be dried or
  • the ZBS-containing residue may then be purified, e.g. by washing it with acid
  • the HC-E solution is in the form of an aqueous
  • the mixture contained 30g concentrated HC-E and 4g HN0 3 in
  • the in situ ZBS may also be formed in the presence of a small quantity of HC£
  • the purified ZBS may then be converted to AZST, e.g. by mixing it with a
  • the wet AZST-containing product may be dried or roasted at a temperature of between 250°C and 450°C, e.g. at about 350°C, and the AZST may be
  • the acid wash solutions (pH approximately
  • the precipitate may be mixed with just enough
  • lime to render an almost dry product, which can be calcined, if desired, for
  • the final washes used to further reduce the level of alkali metal in the wet residue as described above may also be added to the acid wash
  • separated supernatant solutions may be directly disposed of.
  • alkali metal containing compound in mass ratio of 1: 1 to the zircon about
  • zirconium is acid extractable.
  • the product formed may be dried to form a dried residue.
  • the dried residue may also be calcined to form a zircon derived base material
  • zircon derived material suitable for pigments comprises:
  • the process may include the step of preparing of AFDZ and the AFDZ may
  • the AFDZ may be leached with water.
  • the wet residue which forms may still be leached with water.
  • the wet residue which forms may still be leached with water.
  • the wet residue or AFDZ may be neutralised as
  • some silica present in the zircon may be any silica present in the zircon.
  • the process may thus include mixing particulate silica with the calcined product to replenish at least some of the silica leached from
  • the ZBS which forms in situ may be subjected to purification.
  • the process may include a size reduction step, e.g. wet milling, to
  • the ZBS which forms in situ may be subjected to purification.
  • 800°C and 1000°C e.g. about 900°C, and preferably from 1 to 2 hours.
  • the leaching step of the AFDZ may include mixing the AFDZ with NaHC0 3
  • the alkali salt in the alkali salt-containing liquid thus being Na 2 C0 3 .
  • the AFDZ in the AFDZ is leached or washed form the AFDZ. More preferably, at least
  • the zircon derived material is suitable for all zircon-type zirconium pigments
  • ZBS zirconium basic sulphate
  • calcined base material has a typical composition by mass of about 56% Zr0 2 ,
  • Pigments are produced. Pigments may be prepared from the zircon-derived base material using any combination of
  • zircon to produce opacifier material comprises:
  • the process may include subjecting the opacifier material to a size
  • the opacifier material may subsequently be dried at a temperature of about 120°C.
  • containing product may be effected as hereinbefore described.
  • the process may include the formation of AFDZ.
  • the AFDZ may be formed, and leached, as hereinbefore described.
  • process may include recovering at least some of the alkali from the wet residue
  • the process may include subjecting raw zircon to
  • zircon to increase the zirconium content thereof comprises the steps of:
  • ZBC zirconium basic carbonate
  • ZBS solid zirconium basic sulphate
  • the method may include the step of forming the AFDZ, which AFDZ may
  • the AZST solution may be prepared as described hereinbefore.
  • portion is used to convert the hydrated ZBC or hydrated zirconium oxide to
  • the ZBC may
  • the AZST may be formed from the AFDZ as described hereinbefore.
  • final pH of the hydrated ZBC or hydrated zirconium oxide may be between 6,5 and 7, e.g. about 6.75 from the liquid phase.
  • hydrated zirconium oxide may then be separated from the liquid phase and
  • the hydrated ZBC may be washed with water to remove soluble sulphates.
  • hydrated zirconium oxide may be converted to the ZBS by reacting it with
  • a source of sulphate such as H 2 S0 4 or AZST and heating at 80°C for at least
  • the process may include drying the ZBS which forms, e.g. at a temperature
  • the process may also include purifying the ZBS as described hereinbefore.
  • the purified ZBS may be converted to AZST.
  • the invention also relates to products of the processes substantially as
  • the inert composition may comprise a refractory oxide, preferably a ceramic
  • a zirconium containing product preferably it comprises
  • the lining is a AFDZ lining and, the AFDZ lining is preferably
  • the AFDZ lining is about
  • the AFDZ for use as lining Preferably, for elevated temperatures above 650° C, the AFDZ for use as lining
  • the invention also relates to products formed by the processes as described
  • FIG. 1 which shows a schematic flow diagram of a process in accordance
  • reference numeral 10 generally indicates a process in
  • the process 10 includes a raw zircon solids feed line 12 leading to a milling
  • reaction stage 18 an AFDZ feed line feeds a cooling and comminuting stage 22
  • a comminuted AFDZ feed line 24 leads to a leaching stage 26.
  • leachate treating stage 30 is connected by a leachate line 28 to the leaching stage
  • An alkali metal depleted wet residue line 36 leads from the alkali recovery stage
  • the water washing stage 42 is connected to a neutralising stage 38 from where a neutralised wet residue line 40 feeds into a water washing stage 42.
  • the water washing stage 42 is connected to a
  • drying/roasting stage 50 which is connected to an acid leaching stage 54 by
  • An acid leached ZBS-containing product line 56 leads from the acid leaching
  • product line 68 leads from the AZST water extraction stage 66.
  • the neutralised wet residue line 40 also leads to an
  • in situ AZST producing stage 70 which is connected to an AZST
  • dry AZST line 76 leads to a water extraction stage 78 which is connected to a
  • the ZBC precipitating stage 84 by means of an AZST solution line 82.
  • precipitating stage 84 has a ZBC containing product line 86 leading to a
  • a ZBS slurry line 94 leads form the
  • ZBC/ AZST admixing stage 92 to a slurry during stage 96 from where a dry slurry line 98 leads to an acid leaching stage 100.
  • the ZBS-containing product line 48 also leads to a wet residue milling stage
  • a calcined product line 114 leads from the drying/calcining stage 112 to
  • the acid leached ZBS containing product line 56 also leads to a calcining stage
  • a calcined product line 122 leads
  • product line 126 leads.
  • raw zircon solids are fed along the raw
  • a mass ratio between the zircon and the Na 2 C0 3 is about 1 :0,65.
  • the AFDZ is fed along the AFDZ feed line 20 to the cooling and comminuting stage 22,
  • the cooled, comminuted AFDZ is fed along the comminuted
  • AFDZ feed line 24 to the leaching stage 26, where it is leached with water.
  • NaOH may be used in a reaction stage 18
  • sodium silicates and/or precipitated silicas are produced from the leachate by
  • wet residue from the leaching stage 26 is passed along the wet residue line 32
  • the alkali metal depleted wet residue leaves the alkali metal recovery stage 34 along the alkali metal deplete wet residue line 36 and enters the neutralising
  • the washed wet residue is fed by means of the washed wet residue line 44 into
  • H 2 S0 4 (or AZST) is added to the wet residue to convert acid extractable
  • stage 54 where the ZBS containing product is leached with an aqueous mixture
  • stage 58 by means of the acid leached ZBS containing product line 56.
  • the acid leached ZBS containing product is treated
  • the AZST is passed along the AZST product containing line 60 to the
  • AZST drying stage 62 where it is dried at a temperature of about 350°C.
  • dry AZST moves along the dry AZST line 64 to the AZST water extraction
  • stage 66 where the dry AZST is extracted with water to form an AZST
  • the AZST solution may be further treated by methods known to those
  • wet residue from the neutralising stage 38 may be passed to the in situ AZST
  • AZST containing product is thus passed along the AZST containing product
  • AFDZ from stage 22 may be converted directly into AZST by adding
  • Dry AZST is fed along the dry AZST line 76 to the water extraction stage 78,
  • the AZST containing solution may then be further treated/purified by passing
  • a ZBC containing product is then passed along the ZBC containing
  • the ZBS slurry is passed along the ZBS slurry line 94 to the slurry heating
  • stage 96 where it is heated at a temperature of about 80-90°C for at least 10 minutes, whereafter it is fed tot he acid leaching stage 100 along the dry slurry
  • AZST is produced in the same fashion as in the
  • AZST producing stage 58 to produce an AZST product delivered through the
  • the AZST product line 106 The AZST product may be further treated if desired.
  • wet residue is wet milled to have an average particle size which is appropriate
  • the milled residue is fed along the wet milled residue line 110 to the drying/ calcining stage 112, where it is initially dried at a temperature of about
  • stage 116 In the fine silica mixing stage 116, the calcined product is mixed
  • Zircon derived base material is thus delivered
  • Na 2 C0 3 is mixed with NaHC0 3 and water in a washing stage 128, forming a Na 2 C0 3 .
  • the wet residue thus contains
  • the wet residue thus contains
  • containing liquid includes 95% of the alkali salts, as Na 2 C0 3 , that were present
  • opacifier material is a material that is milled to achieve a d 50 particle size of less than 1.5 ⁇ m.
  • AFDZ was prepared using zircon powder with a d 50 particle size of 6,5 ⁇ m
  • AZST formed were water-leached and the solutions separated from the
  • AFDZ was prepared using zircon powder with a d 50 particle size of 6.5 ⁇ m
  • zirconyl chloride from which ZBS is precipitated using (NH 4 )S0 4 as precipitating agent.
  • the ZBS was separated, washed with water, then dried,
  • An AZST solution was prepared from the AZST obtained from the in situ ZBS
  • resin column (resin Duolite A161L Code 60393, obtained from Rohm and
  • the zircon alkali metal containing compound mass ratio for all the
  • the AZST-containing product was roasted to dryness at
  • the ZBS-containing slurry was purified with HC-E/HN0 3 solutions as
  • AFDZ was prepared using zircon flour (95% ⁇ 45 ⁇ m) and NaOH and the
  • ZBS precipitate was oven dried, calcined at 900°C, wet milled to a d 50 particle
  • this opacifier was 83% based on the starting mass of the zircon flour used.
  • impurity elements particularly iron, uranium and calcium

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Inorganic Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Metallurgy (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Geology (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

L'invention concerne un procédé de traitement de produits contenant du zirconium, tels que le zircon. Ledit procédé comprend la formation d'un produit du zircon décomposé par fusion d'alcalis (AFDZ), obtenu en traitant le zircon avec une source de métaux alcalins à des températures élevées. Le zircon décomposé par fusion avec des métaux alcalins (AFDZ) est ensuite traité pour former un solide contenant de l'oxyde de zirconium hydraté et/ou du carbonate basique de zirconium hydraté (appelé produit de zirconium hydraté ci-après). Ledit procédé comprend également le traitement du produit de zirconium hydraté solide pour la formation in situ de sulfate de zirconium basique solide. L'invention concerne également : un tel procédé de production de dérivés du zircon, utilisables comme pigments ; un tel procédé de production de matériaux opacificateurs ; et les produits obtenus par ces procédés.
PCT/ZA2000/000104 1999-06-07 2000-06-06 Enrichissement du zircon Ceased WO2000075075A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
US10/009,110 US7063824B1 (en) 1999-06-07 2000-06-06 Beneficiation of zircon
AU56437/00A AU5643700A (en) 1999-06-07 2000-06-06 Beneficiation of zircon

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
ZA99/3815 1999-06-07
ZA993815 1999-06-07

Publications (1)

Publication Number Publication Date
WO2000075075A1 true WO2000075075A1 (fr) 2000-12-14

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Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/ZA2000/000104 Ceased WO2000075075A1 (fr) 1999-06-07 2000-06-06 Enrichissement du zircon

Country Status (3)

Country Link
US (1) US7063824B1 (fr)
AU (1) AU5643700A (fr)
WO (1) WO2000075075A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2936514A1 (fr) * 2008-09-30 2010-04-02 Saint Gobain Ct Recherches Poudre d'hydrate de zirconium

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2005116277A1 (fr) * 2004-05-27 2005-12-08 The South African Nuclear Energy Corporation Limited Valorisation du zircon
CN107531508B (zh) * 2015-02-09 2021-01-08 艾绿卡资源有限公司 提高锆石等级和光学质量的方法
JP6766074B2 (ja) * 2016-01-05 2020-10-07 住友電気工業株式会社 金属成分の分離方法

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3672825A (en) * 1970-02-16 1972-06-27 Tizon Chem Corp Process for preparing basic zirconium sulfates and other zirconium compounds such as zirconium fluosulfates,and compositions containing the same
WO1986004614A1 (fr) * 1985-02-01 1986-08-14 Commonwealth Scientific And Industrial Research Or Procede de production de zircone tres pure
WO1988003128A1 (fr) * 1986-10-28 1988-05-05 Commonwealth Scientific And Industrial Research Or Procede de production de sulfate de zirconium

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1376161A (en) * 1919-01-30 1921-04-26 Pennsylvania Salt Mfg Co Process of making basic zirconium sulfate
EP0210236A4 (fr) * 1985-02-01 1988-01-07 Commw Scient Ind Res Org Procede de production de zircone tres pure.

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3672825A (en) * 1970-02-16 1972-06-27 Tizon Chem Corp Process for preparing basic zirconium sulfates and other zirconium compounds such as zirconium fluosulfates,and compositions containing the same
WO1986004614A1 (fr) * 1985-02-01 1986-08-14 Commonwealth Scientific And Industrial Research Or Procede de production de zircone tres pure
WO1988003128A1 (fr) * 1986-10-28 1988-05-05 Commonwealth Scientific And Industrial Research Or Procede de production de sulfate de zirconium

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
RALPH NIELSEN: "Zirconium and Zirconium Compounds", ULLMANN'S ENCYCLOPEDIA OF INDUSTRIAL CHEMISTRY, vol. a, no. 28, 1996, Weinheim, pages 543 - 567, XP002146764 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2936514A1 (fr) * 2008-09-30 2010-04-02 Saint Gobain Ct Recherches Poudre d'hydrate de zirconium

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Publication number Publication date
US7063824B1 (en) 2006-06-20
AU5643700A (en) 2000-12-28

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